#------------------------------------------------------------------------------
#$Date: 2025-08-20 22:19:29 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/65/4306560.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306560
loop_
_publ_author_name
'Stuart D. Robertson'
'Tristram Chivers'
'Heikki M. Tuononen'
_publ_contact_author_address
;
Department of Chemistry
University of Calgary, Calgary, Alberta 
T2N 1N4, Canada
;
_publ_contact_author_name        'Prof. T. Chivers'
_publ_section_title
;
Experimental and Theoretical Investigations of the Redox Behavior of the
Heterodichalcogenido Ligands [(EPiPr2)(TePiPr2)N]-(E = S, Se): Cyclic
Cations and Acyclic Dichalcogenide Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10634
_journal_page_last               10643
_journal_paper_doi               10.1021/ic801384c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C24 H56 N2 P4 Se2 Te2'
_chemical_formula_sum            'C24 H56 N2 P4 Se2 Te2'
_chemical_formula_weight         909.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.4738(16)
_cell_angle_beta                 96.350(2)
_cell_angle_gamma                92.604(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5584(2)
_cell_length_b                   8.0137(3)
_cell_length_c                   15.0009(5)
_cell_measurement_reflns_used    12960
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     893.72(5)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'nonius KappaCCD'
_diffrn_measurement_method       'phiω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15765
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    3.864
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0264P)²+0.7718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                3430
_reflns_number_total             4025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801384c_si_001_4.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4306560
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.99107(3) 0.55253(3) 0.910998(13) 0.02539(8) Uani 1 1 d . . .
Se1 Se 0.99161(4) 0.62705(4) 0.69865(2) 0.02733(9) Uani 1 1 d . . .
P1 P 1.08479(9) 0.28115(9) 0.83524(5) 0.01684(16) Uani 1 1 d . . .
P2 P 1.18531(10) 0.44053(10) 0.68088(5) 0.01968(16) Uani 1 1 d . . .
N1 N 1.1883(3) 0.3046(3) 0.75145(16) 0.0221(5) Uani 1 1 d . . .
C10 C 0.8890(4) 0.1324(4) 0.8045(2) 0.0245(7) Uani 1 1 d . . .
H10A H 0.9263 0.0350 0.7636 0.029 Uiso 1 1 calc R . .
C11 C 0.8239(4) 0.0608(4) 0.8856(2) 0.0330(8) Uani 1 1 d . . .
H11A H 0.7152 -0.0118 0.8655 0.050 Uiso 1 1 calc R . .
H11B H 0.7983 0.1536 0.9308 0.050 Uiso 1 1 calc R . .
H11C H 0.9165 -0.0053 0.9126 0.050 Uiso 1 1 calc R . .
C12 C 0.7360(4) 0.2083(5) 0.7510(2) 0.0360(8) Uani 1 1 d . . .
H12A H 0.6464 0.1185 0.7238 0.054 Uiso 1 1 calc R . .
H12B H 0.7822 0.2638 0.7031 0.054 Uiso 1 1 calc R . .
H12C H 0.6813 0.2911 0.7917 0.054 Uiso 1 1 calc R . .
C20 C 1.2323(4) 0.1886(4) 0.91802(18) 0.0175(6) Uani 1 1 d . . .
H20A H 1.1641 0.1688 0.9695 0.021 Uiso 1 1 calc R . .
C21 C 1.2869(4) 0.0175(4) 0.8746(2) 0.0267(7) Uani 1 1 d . . .
H21A H 1.3629 -0.0337 0.9195 0.040 Uiso 1 1 calc R . .
H21B H 1.3527 0.0338 0.8233 0.040 Uiso 1 1 calc R . .
H21C H 1.1799 -0.0567 0.8532 0.040 Uiso 1 1 calc R . .
C22 C 1.3956(4) 0.3045(4) 0.9556(2) 0.0263(7) Uani 1 1 d . . .
H22A H 1.4669 0.2535 1.0024 0.039 Uiso 1 1 calc R . .
H22B H 1.3578 0.4135 0.9820 0.039 Uiso 1 1 calc R . .
H22C H 1.4676 0.3212 0.9066 0.039 Uiso 1 1 calc R . .
C30 C 1.1492(4) 0.3201(4) 0.5671(2) 0.0299(7) Uani 1 1 d . . .
H30A H 1.1590 0.4019 0.5226 0.036 Uiso 1 1 calc R . .
C31 C 0.9639(5) 0.2323(5) 0.5472(2) 0.0375(8) Uani 1 1 d . . .
H31A H 0.9446 0.1799 0.4838 0.056 Uiso 1 1 calc R . .
H31B H 0.8744 0.3150 0.5580 0.056 Uiso 1 1 calc R . .
H31C H 0.9531 0.1453 0.5868 0.056 Uiso 1 1 calc R . .
C32 C 1.2920(5) 0.1934(5) 0.5527(2) 0.0410(9) Uani 1 1 d . . .
H32A H 1.2670 0.1293 0.4920 0.061 Uiso 1 1 calc R . .
H32B H 1.2913 0.1159 0.5981 0.061 Uiso 1 1 calc R . .
H32C H 1.4094 0.2538 0.5588 0.061 Uiso 1 1 calc R . .
C40 C 1.4114(4) 0.5388(4) 0.6910(2) 0.0245(7) Uani 1 1 d . . .
H40A H 1.4936 0.4454 0.6816 0.029 Uiso 1 1 calc R . .
C41 C 1.4357(5) 0.6523(5) 0.6185(3) 0.0461(10) Uani 1 1 d . . .
H41A H 1.5601 0.6967 0.6250 0.069 Uiso 1 1 calc R . .
H41B H 1.3575 0.7462 0.6256 0.069 Uiso 1 1 calc R . .
H41C H 1.4052 0.5870 0.5584 0.069 Uiso 1 1 calc R . .
C42 C 1.4672(4) 0.6321(4) 0.7858(2) 0.0307(7) Uani 1 1 d . . .
H42A H 1.5929 0.6722 0.7912 0.046 Uiso 1 1 calc R . .
H42B H 1.4512 0.5556 0.8306 0.046 Uiso 1 1 calc R . .
H42C H 1.3934 0.7285 0.7966 0.046 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Te1 Te1 95.01(3) . 2_767 ?
N1 P1 C20 108.49(13) . . ?
N1 P1 C10 112.24(14) . . ?
C20 P1 C10 105.90(14) . . ?
N1 P1 Te1 112.66(10) . . ?
C20 P1 Te1 108.05(9) . . ?
C10 P1 Te1 109.20(10) . . ?
N1 P2 C40 106.98(14) . . ?
N1 P2 C30 106.64(15) . . ?
C40 P2 C30 105.18(15) . . ?
N1 P2 Se1 114.67(9) . . ?
C40 P2 Se1 111.29(11) . . ?
C30 P2 Se1 111.51(12) . . ?
P1 N1 P2 134.06(16) . . ?
C12 C10 C11 110.5(3) . . ?
C12 C10 P1 112.1(2) . . ?
C11 C10 P1 113.4(2) . . ?
C22 C20 C21 110.8(2) . . ?
C22 C20 P1 112.1(2) . . ?
C21 C20 P1 109.4(2) . . ?
C31 C30 C32 110.7(3) . . ?
C31 C30 P2 111.8(2) . . ?
C32 C30 P2 111.6(2) . . ?
C42 C40 C41 111.5(3) . . ?
C42 C40 P2 111.4(2) . . ?
C41 C40 P2 112.8(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 P1 2.4896(10) . ?
Te1 Te1 2.8935(8) 2_767 ?
Se1 P2 2.1518(10) . ?
P1 N1 1.579(2) . ?
P1 C20 1.829(3) . ?
P1 C10 1.836(3) . ?
P2 N1 1.614(3) . ?
P2 C40 1.831(3) . ?
P2 C30 1.834(3) . ?
C10 C12 1.529(4) . ?
C10 C11 1.530(4) . ?
C20 C22 1.520(4) . ?
C20 C21 1.534(4) . ?
C30 C31 1.520(5) . ?
C30 C32 1.528(5) . ?
C40 C42 1.524(4) . ?
C40 C41 1.526(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 102031389
